Process of and apparatus for cleaning wool.



No. 630,293. I Patented Aug. I, I899. E. MAERTENS.

PROCESS OF AND APPARATUS FOR CLEANING WOOL. (Application filed June 24,1899.) (No Model.)

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UNrrnD STATES PATENT @FFICE.

EMILE MAERTENS, OF PROVIDENCE, RHODE ISLAND.

PROCESS OF AND APPARATUS FOR CLEANING WOOL.

' SPECIFICATION forming part of Letters Patent No. 630,293, dated August1, 1899.

Application filed June 24,1899. Serial No. 721,730. (No model.)

To ail whom it may concern-.-

Be it known that l, EMILE MAERTENS, a citizen of the United States,residing at Providence, in the county of Providence and State of RhodeIsland, have invented certain new and useful improvements in the art ofcleaning wool and other animal fibers with volatile solvents, the objectbeing to obtain the wool or fiberin the best workable condition and torecover the by-products, such as wool-fat and the potash, of which thefollowing is a specification.

The invent-ion relates to a process of and apparatus for the extractionof oily, greasy, resinous, and other substances from wool and othermaterial and is especially designed for use in establishments where theoutput does not warrant the necessary expenditure for the more elaborateprocesses and apparatus described in my United States Patents Nos.545,899, 545,900, and 615,030.

Referring to the accompanying drawings, Figure 1 is a general elevationof the apparatus with the digester shown in section. Fig. 2 is a detailof the digester-cover, and Fig. 3 is a detail of the hydraulic plungerwith its perforated extension or platen.

A is the digester, wherein the material to be extracted is placed,either while contained in a cage or basket or loose, and'is supposed tobe provided with suitable doors 0r covers for loading and unloading thematerial and closing the apparatus. It can also be of the specialconstruction shown herein, which consists of the straight cylindricalpart a, carry ing at its top an enlarged annular chamber a, adapted forthe reception of a cover I) and of heating-coils c, and at its bottom asomewhat similar enlarged annular chamber a adapted for the reception ofheating-coils o and of a hydraulic ram d, having a Watertight packing ate. The cover 1) consists of the solid cap part b and of the foraminoushollow extension 19 .The ram (Z, which is shown in detail in Fig. 3,consists of the plunger d, adapted to slide in the extension a ofchamber a and of the foraminous hollow extension or platen (1 which isfastened to it.

Bis a reservoir provided with suitable heating-coils for the solventused in the process and when in use generally contains solvent having acertain amount of extracted matter in solution.

C is a condenser or cooler of any suitable construction for the coolingof liquids or the condensation of vapors.

D is a heater of any suitable construction for the heating orsuperheating of gases or vapors.

E is a vacuum-pump adapted for use also as an air or gas circulatingpump, and it is connected by suitable valved piping with all the otherelements of the apparatus.

F is an oil condenser or extractor uscdfor the retention or condensationof the solvent vapors contained in the air which is allowed to escapeinto the atmosphere and may be provided with heating means for thevolatilization of the solvent retained by the oil in said condenser.

G and II are drums or reservoirs provided with heating-coils and areadapted for the reception of liquids, for their separation, volatilization, or evaporation.

The various elements of the apparatus are provided wherever necessarywith suitable valved inlet and outlet pipes, as well as with gages,drain-cocks, thermometers, sightglasses, (to.

The method for operating the apparatus is as follows, the material to beextracted or treated being supposedly raw wool: The digester A havingbeen charged with the Wool to be extracted (in space a) and hermeticallysealed, by preference, and in order to insure a perfect penetration ofthe solvent to be used to all parts of the mass to be treated a vacuumis created in the digester A by putting the latter in communication withthe pump E through valve 1, pipes 100 and 101', and valve 2. The airexhausted is discharged into the atmosphere through pipe 102 and valve3. When a suitable vacuum has been obtained, the pump E is stopped, andthe valves previously opened are again closed. Steam having been turnedonto the coils in reserv'oirB by opening valve e1: on pipe 103, thepressure soon rises in this tank through the tension of the vapors ofthesolventvolatilized by the heat of the coils,and when the internalpressure becomes sufficient valve 6 on pipe 104,valves 7, 8, and 9 onpipe 105, and valve 10 on pipe. 106 are opened, or if the solvent isjudged to be too hot it is first put through the cooler or condenser 0via pipe 107, valve 11, pipe 108, and valve 12, and from the condenserenters pipe 105 by way of valve 13 on pipe 109 and valve 14 on pipe 110.When driving the solvent into pipe 105 by way of the condenser O, valve7 on pipe 105 must of course be closed. The solvent containing extractedwool-fat in solution from preceding operations is now forced from thebottom of the tank B through the pipes and valves just mentioned intothe top of the digester A, which is filled therewith. Should a vacuumnot have been made in the digester prior to the admission of thesolvent, the latter is preferably allowed to enter at the bottom of thedigester by valve 38, the air displaced by the solvent being allowed toescape by opening valves 2 and 15 on pipe 101 and valve 16 on pipe 111and enter the oil-condenser F through check-valve 17, where in passingthrough the oil contained therein it is stripped of the solvent vaporswith which itis charged before escaping into the atmosphere throughvalve 18 on pipe 112, or it can first be passed through the condenser Cand-from there to the condenser F by way 'of valves 19 and 20 on pipe113, valve 21 on pipe 114, pipe 115 and valve 22, and checkvalve 17 onpipe 111. The digester A being now full of solvent containing wool-fatin solution valve 6 on pipe 104 is closed, valve 23 on pipe 116 isopened, and valve 7 on pipe 105 is closed. The solvent vapors generatedin reservoir B now rise through pipes 116, 104, 107, valve 11, pipe 108,and valve 12 and enter the condenser through pipe 114, from which theyemerge in liquid form through pipe 109, and from there the pure solvententers the top of digester A through valve 13, pipe 110, valve 14, pipe105, and valves 8, 9, and 10, valve 38 being closed. Valve 24 on pipe117 and valve 25 on pipe 119 are now opened and the charged solventcontained in digester A is allowed to return to tank B through pipe 117,118, and 119, care being taken by throttling valves 24 or 25 not to letthe charged solvent from the bottom of digester A into tank B any fasterthan the pure solvent from condenser O enters digester A at its top, andthus a complete continued immersion of the material being extracted isinsured. If desired, the solvent from the digester can be run into drumsH or G by opening valves 28 or before being returned to tank B. \Vhenthe whole of the material contained in digester A has been sufficientlyrinsed with the pure solvent coming from condenser O, valve 11 on pipe107 is closed, as well as valves 12 and 13 on the inlet and the outletto the condenser C and valve 8 on pipe 105, whereas valve 7 on pipe 105,Valve 26 on pipe 109, and valve 27 on pipe 120 are opened, valve 14 onpipe 110 not having been closed. Meanwhile all the liquid solventcontained in the digester A having been drained into tank B valve 25 onpipe 1'19 is closed. The vapors generated in B now pass into the heaterD, where they are superheated, and from there through valve 10 into thetop of the digester, or they can be sent direct from pipe 104 into pipe105 through valves 7, 8, 9, and 10 and be superheated in the chamber aby the coils 0. These superheated vapors, which are under pressure,somewhat compress the whole mass of wool and at the same time heat it upto the point of vaporization of the residual solvent which it contains,and upon opening valve 28 on pipe 121 leading into drum G a quantity ofliquid solventis discharged into said drum, whereas vaporized solventascends pipe 122 into pipe 101 and from there enters the condenser byway of valve 15, pipe 113, valve 19, pipe 108, valve 12, and pipe 114and when condensed is delivered into drum H or G via valve 29 on pipe123 and valves 30 and 31. This operation is continued untilsubstantially all the residual solvent has been removed from thematerial. I have found by experience that the wool is liable to beinjured if in the treatment thereof the temperature is allowed to goabove 60 centigrade. The exact temperature will vary with differentwools as well as with the nature of the solvent employed. Thetemperature which I prefer to employ in driving off the residual solventfrom the wool is from to centigrade. Valves 4, 23, 9, and 28 are nowclosed, steam is turned on at valve 32 on pipe 106 for a few seconds,and this completely removes the last traces of solvent and deodorizesthe material, which is now dry and degreased and in condition forremoval from the digester in anysuitable manner after atmospheric airhas been circulated through the material in order to cool it off. Thisis done by closing all valves previously opened, starting up thevacuum-pump, and opening valve 3 on pipe 102, valve 1 on pipe 100, valve2 on pipe 101, and valve 33 on pipe 124. This latter valve 33 admitsatmospheric air, which is drawn through the mass and discharged into theatmosphere either through valve 3 or by way of the oil-condenser F viavalves 34 and 22 on pipe 115 and valve 18 on pipe 112 or by way ofcondenser C and the oil-condenser F, as previously described.

The removal of residual solvent by the aid of superheated solvent vaporsalone is a tedious and dangerous operation, which, unless carried onwith great care and judgment, is very liable toinj ure the materialbeing treated when this is wool, and is not to be recommended even ifcarried on by very experienced and careful operators.

The removal of the residual solvent is much accelerated, the quality ofthe work is much improved, and the danger of injury to the material verymaterially removed by the use of a vacuum-pump or of steam inconjunction with solvent vapors or by a combination of two or of allthree of the elements mentioned.

When steam is used with or without the vacuum-pump, a small jet of it isadmitted to pipe 106 by valve 32, where it mixes with the solvent vaporsbefore they enter the digester, the water resulting from thecondensation of the steam being separated from the solvent in drums H orG.

When the vacuum-pump is used with solvent vapors or with steam or withboth solvent vapors and steam for the removal of the residual solvent,valve 28 on pipe 121 is closed, and all other valves being open or shut,as required, the vapors are circulated from the bottom of the digesterthrough valve 24 on pipe 117, through pipes 122 101 100, and throughvalve 1, and are discharged by the pump E into condenser C via pipe 102,valve 34, pipe 115, and valve 21 on pipe 114, the liquefied vaporsfinding their'way into drums H or G via pipe 109, valve 29, pipe 120,and valves 30 or 31.

In lieu of solvent vapors water vapors are sometimes used for theremoval of the residual solvent, and when this is the case valve 24 onpipe 117 is closed and the bottom chamber a of the digester is filled orpartially filled with Water by opening valves 35 and 36 on pipe 125.Steam is turned on to coils c of chamber a by opening valve 37. Valve 2on pipe 101 and valve 1 on pipe 100 being opened and the vacuum-pumpstarted, under the influence of the vacuum produced and the heattransmitted by coils c the water in chamber a is vaporized and drawnthrough the contents of the digester, heating it up and vaporizing theresidual solvent, which, along with the water-vapors, is delivered bythe pump E into condenser C and from there into drums H or G, aspreviously described.

In lieu of water-vapors, of steam, of solvent vapors, or a combinationof two or three of the above with or without a vacuum, the residualsolvent is sometimes removed by air which is circulated over and overagain through the material, preferablyin conjunction with steam. Thenthis is practiced, air is allowed to enter the system by valve 33 onpipe 124 or by any other inlet or inlets suitably sitnated for thepurpose, and the pump E is started. If desired, the air may beindirectly heated prior to its introduction into the digester or may bedirectly heated by mixing steam therewith. The air is drawn through thematerial and emerges from the digester through valve 2 on pipe 101,enters the pump through valve 1 on pipe 100, leaves the pump throughpipe 102, enters the condenser through valve 34 on pipe 115 and valve 21on pipe 114, passes through the condenser, leaving behind solvent andwater vapors, which are condensed and run to tanks H or G, via valve 29on pipe 123 and valves 30 or 31, and through pipe 109 and valves 13 and20 enters the heater D, where it absorbs heat, emerges from the latterthrough pipe 120, enters pipe 105 through valve 27 and pipe 106 throughvalve 9. In pipe 106 it is preferably mixed with steam injected throughvalve 32 and reenters the bottom chamber a of digester A through valve33. This air is thus circulated in a cycle, recooled, reheated, andremixed with steam until all of the residual solvent contained in thematerial held by the digester has been removed, and it is thendischarged into the atmosphere by way of the oil-condenser, aspreviously described.

In order to accelerate the removal of the residual solvent and beforethe circulation of steam, air, or vapors through the material, thelatter can be squeezed for the expression of the bulk of the residualsolvent. This is accomplished by making use of the ram (1, (or of anyequivalent device or means,) which on being raised by the mediumactuating it compresses the material between the hollow foraminousplaten d and the hollow forami nous extension 6 of the cover I), theliquid expressed escaping through the perforations of said platen andcover into chambers a and d and emerging from there, through valves 10and 38 on pipe 106 and valves 24 and 28 on pipes 11.7 and 121, into drumG. When the liquid has been expressed as described, the ram is againallowed to drop, and the re moval of the still-adherim solvent iscarried on as previously described.

It is obvious that after treating the material and removing the cover I)the digester can be emptied by the action of the plunger (1, which, whenraised, carries with it the hollow foraminous platen d and all that issupported by the latter to the top of the digesterA, where it is caredfor in any suitable manner.

When the material being extracted is going to be subjected to asubsequent Wet treat ment in the digester itself, it is convenient toremove the residual solvent by means of the liquid or solution withwhich the material is to be treated or with water, provided these areimmiscible with the solvent used in the extraction, and the operation isthen as follows: Assuming that the liquid to be used is water and thatthe material is to be partially prepared for carbonizing or entirelycarbonized in the digester A and that the bulk of the residual solventhas or has not been re moved by compression, as described above, waterof a suitable temperature is allowed to enter digester A via valve 36,pipe 125, valve 35, and chamber a (it can, if need be, be heated bycoils c in said chamber) and to rise slowly in the part (1, containingthe extracted material. The adhering solvent is thereby nearly allremoved and floated on top of the water or solution used. WVhen thefloating solvent reaches chamber 11 the inlet-flow of water is reducedor stopped, steam is turned on the coil 0 by opening valve 39, and thefloating solvent distilled off either in 'vacuo, the vapors goingthrough valves 2 and 1 and the pump on their way to the condenser, ordirect to the condenser via valve 2, pipe 101,

valve 15, pipes 104 and 113, valve 19, pipe 108,

and valve 12, or the solvent can be floated 0ft slowly into drums H or Gvia valve 2, pipes 122 117, and valves 28 or 40. When the soladheringcarbonizing solution.

ventwhich has floated to the top has been removed, valve 2 is closed andthe material is compressed by moving plunger d upward, as previouslydescribed. This liberates further traces of solvent and also the naturalsoaps or potash salts contained in the wool and which had dissolved inthe surrounding liquid. The floating solvent is fioated'off or distilledoif, as previously described, and the liquid containing the potash saltsin solution is run into drums H or G by way of valves 10 and 38 on pipe106 and valve 24, pipe 117, and valves 28 or 40 for the removal oftraces of solvent, or it is run direct to a storage-tank by way of valve33 on pipe 124 for reuse or until its concentration warrants itsvaporization for the recovery of the potash salts or other extractedmaterial held in solution. The material can now after a slight steamingbe removed from the digester and carried to the washers to be rinsed forthe removal of extraneous impurities, or it can be further rinsed in thedigester itself by repeated immersions, compressions, and changes ofwater, and this is the case when it is desired to prepare the materialfor carbonizing or when it is desired to carbonize the material in thedigester itself or to remove it from the digester cleansed or cleansedand dried. I

In order to prepare the material for car- ,bonizing after it has beensufficiently rinsed,

it is finally compressed and the water allowed to drain out of thedigester through valve 33 on pipe 124. The plunger d is then allowed todrop, and after closing valve 33 the carbonizing solution is introducedthrough valves 41 and 35 on pipe 125 and chamber (t into the part a ofdigester A,when the material contained therein is completelyimmersed bythe solution, the flow is stopped, and the material is allowed to steepfor a suitable period. The solution is then allowed to return to itsstorage-tank through valve 33 on pipe 124, and the plunger d is made tocompress the material for the removal of the bulk of the The materialcan now be removed to be dried, carbonized, neutralized, and redried, orit can be dried by passing steam and hot air through it in the mannerpreviously described and when dry carbonized by eliminating the steamfrom the circulation and increasing the temperature of the circulatingair in the heater D and in coils c and c. When the carbonization iscomplete, the material can be neutralized in the same manner that it wasprepared for the carbonization by merely changing the solution used. Itcan then be rinsed with water and after being pressed for the removal ofthe bulk of adhering moisture dried with hot air and steam, aspreviously described, when it will be found in a finished and cleancondition ready to be thrown out of the digester by operating theplunger d. The liquids accumulated in drums H and G are separated bydecantation or evaporation, or by both, the

drums being suitably connected with the condenserO and tank B, as wellas with the drain and with storage-tanks for this purpose.

If desired, the material can be treated with water in the digester afterthe residual solvent has been removed by superheated solvent vapors,water-vapors, air or steam, or both, or a combination of any of themeans mentioned. If this water treatment is done thoroughly in the caseof some wools, so as to remove all potash soaps present, and the wool isthen partially dried, it'can then in many cases be freely carded, and anexpensive process can thus be saved.

When the solvent in tank 13 becomes too much saturated with extractedfat, a part of it is run to a still, where the fat is separated from thesolvent. The solvent is then returned to tank B by way of the condenser0 direct or by way of condenser C and drums H and Gin case the solventis mixed with water and needs separating in said drums.

It is evident from thedescription and draw in gs that, if desired, theliquids, gases, or vapors used in the process can be passed through thedigester in either direction when it is deemed advisable or necessary toso do. It is evident that the vacuum-pump can be dispensed with, ifnecessary, in some of the the operations described and that the suctionor vacuum created by the condensation of the vapors in the condenserwill to a great extent accomplish the same object. It is further evidentthat when the solvent used in the process is heavier than the extractedmatter its flow through the digester should be upward, whereas when thesolvent is lighter than the extracted matter its flow should be downwardand that in case of the removal of the residual solvent with a liquidthe flow of the liquid should be downward if the solvent is heavier thanthe liquid used for its removal and that the flow of said liquid shouldbe upward through the digester when the solvent is lighter than theliquid used for its removal.

The method hereinbefore described of removing residual solvent by thecirculation of air in a closed circuit is made the subjectmatter of myapplication Serial No. 721,731, filed concurrently herewith.

The described method of removing residual solvent by aqueous vapor isclaimed in my application Serial No. 721,732.

The described method of removing residual solvent by the inflow of wateris claimed in my application Serial No. 721,733.

Having described my invention, what I claim is 1. The process ofremoving residual solvent from wool after the grease has been extractedtherefrom which consists in subjecting it to the action of superheatedsolvent vapors at a temperature below 100 centigrade, substantially asdescribed.

2. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in first removing ICC theexcess of solvent therefrom by pressure and then subjecting it to theaction of superheated solvent vapors at a temperature below 100centigrade, substantially as described.

- 3. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in subjecting it to theaction of superheated solvent vapors at a temperature below the point atwhich the fiber would be injured by heat, substan tially as described.

4. Theprocess of removing residual solvent from wool after the greasehas been extracted therefrom which consists in subjecting it to theaction of superheated solvent vapors at a temperature below the point atwhich the fiber would be injured by the heat, and then drying the same,substantially as described.

5. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in first removing the excessof solvent therefrom by pressure and then subjecting it to the action ofsuperheated solvent vapors at a temperature below 100 centigrade inconjunction with steam or aqueous vapor, substantially as described.

6. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in subjecting it to theaction of superheated solvent vapors at a temperature below the point atwhich the fiber would be injured by heat in'conjunction with steam oraqueous vapor, substantially as described.

7. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in first removing the excessof solvent therefrom by pressure and then subjecting it to the action ofsuperheated solvent vapors at a temperature below 100 centigradeinconjunction with a vacuum,

substantially as described.

8. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in subjecting it to theaction of superheated solvent vapors at a temperature below the point atwhich the fiber would be injured by the heat in conjunction with avacuum, substantially as described.

9. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in first removing the excessof solvent therefrom by pressure and then subj ectin git to the actionof superheated solvent vapors at a temperature below 100 centigradeinconjunction with steam or aqueous vapor and a vacuum, substantially asdescribed.

10. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in subjecting it to theaction of superheated solvent vapors at a temperature below the point atwhich the fiber would be injured by the heat in conjunction with steamor aqueous vapor and a vacuum, substantially as described.

11. The process of removing residual solvent from wool after the greasehas been extracted therefrom which consists in subjecting it to theaction of superheated solvent vapors at a suitable temperature and inconjunction With or without steam, aqueous vapors or a vacuum, thendeodorizing it and then airing or cooling it, substantially asdescribed.

13. The process of cleaning wool in a digester which consists in firstremoving the fat therefrom by a volatile solvent, eliminating theresidual solvent therefrom with superheated solvent vapors at atemperature not exceeding 100 centigrade, and then depotashing the same,substantially as described.

14. The process of cleaning wool in a digester which consists in firstremoving the fat therefrom by a volatile solvent, eliminating theresidual solvent therefrom with super-' heated solvent vapors at atemperature not exceeding 100 centigrade, depotashing it and thenrinsing it, substantially as described.

15. The process of cleaning wool in a digester which consists in firstremoving the fat therefrom by volatile solvents, eliminating theresidual solvent therefrom with superheated solvent vapors at atemperature not exceeding 100 centigrade, depotashing it, rinsing it,and then drying it, substantially as described.

16. The process of cleaning and treating wool in a digester whichconsists in first removing the fat therefrom, by volatile solvents,eliminating the residual solvent therefrom, depotashing and rinsing itand then subjecting it to the act-ion of a carbonizing solution,substantially as described.

17. The process of cleaning and treating wool in a digester whichconsists in first removing the fat therefrom by volatile solvents,eliminating the residual solvent therefrom, depotashing and rinsing it,subjecting it to the action of a carbonizing solution and then dryingand carbonizing it, substantially as described.

18. The process of cleaning and treating wool in a digester whichconsists in first removing the fat therefrom by volatile solvents,eliminating the residual solvent therefrom, depotashing and rinsing it,subjecting it to the action of a carbonizing solution, drying andcarbonizing it and then neutralizing the carbonizin g agent,substantially as described.

19. The process of cleaning and treating wool in a digester whichconsists in first removing the fat therefrom by volatile solvents,eliminating the residual solvent therefrom, depotashing and rinsing it,subjecting it to the action of a carbonizing solution, drying 1substantially as described.

20. An apparatus for cleaning wool consisting of a digester, asolvent-tank, a settling or separating tank, a surface condenser, aheater or superheater and a vacuum or circulating pump, substantially asdescribed.

21. An apparatus for cleaning wool consisting of a digester, asolvent-tank, a settling or separating tank, a surface condenser, anoilcondenser,and a vacuum or circulating pump,

I substantially as described.

' 22. A digester for use in cleaning Wool by means of volatile solventsprovided with a hydraulic piston adapted for the expression of liquidsfrom the material under treatment, and a cover with a cage attachedthereto having its bottom and sides perforated, substantially asdescribed.

23. A digester for use in cleaning wool by means of volatile solventsprovided with a hydraulic piston having a foraminous platen attachedthereto and adapted for the expression of liquids from the materialunder treatment, and a cover with a cage attached thereto having itsbottom and sides perforated, subi stantially as described.

24. Adigester for use in wool-cleaning,having an enlarged chamber at itstop provided with coils, substantially as described.

25. Adigester for use in wool-cleaning having an enlarged chamber at itstop provided with coils, and a similar chamber at its bottom, providedwith coils, substantially as described.

26. A digester having an enlarged chamber at its bottom provided withcoils and a foraminous platen adapted to compress the material undertreatment, substantially as described.

27. A digester having an enlarged upper portion forming a chamber,heating coils therein, and a foraminous false bottom adapted to beoperated to compress the material under treatment, substantially asdescribed.

28. A digester having an enlarged chamber at its bottom provided withcoils, a perforated false bottom or platen adapted to compress thematerial under treatment, and acover provided with a dependingforaminous chamber, substantially as described.

29. A digester with enlarged upper and lower portions forming chambersexterior to the main body of the digester, coils in said chambers, andmeans for compressing the material under treatment, substantially asdescribed. 30. The process of removing residual solvent from Wool whichconsists in subjecting it to the action of superheated solvent vapors atatemperature not exceeding 60 centigrade, substantially as described.

EMILE MAERTENS. Witnesses:

MABEL I. FAY, RUFUs S. MATTESON.

